Preparation method of high-quality anhydrous rare earth chloride and bromide

A rare earth chloride and bromide technology, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of easy deliquescence, high cost, and difficult dehydration of finished products, and achieve easy industrial production, avoid pollution, and reduce process costs low effect

Inactive Publication Date: 2019-12-06
TIANJIN BAOGANG RES INST OF RARE EARTHS
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  • Summary
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the difficulty in dehydration of these materials, oxyhalides are easily formed during the dehydration process, and the finished products are easily deliquescent, which brings great difficulties to the preparation, packaging, storage, and crystal growth of raw materials.
At present, high-pur

Method used

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  • Preparation method of high-quality anhydrous rare earth chloride and bromide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 1 kg of lanthanum bromide heptahydrate, heat it to 180°C under the protection of flowing nitrogen, and keep it for 3h; vacuumize the system, continue to heat up to 245°C and keep it for 5h, to obtain crude anhydrous lanthanum bromide; Transfer to a vacuum distillation device, after vacuuming (the vacuum pressure is 120Pa at this time), heat up to 260°C for 5h, continue to heat up to 500°C for 4h, continue to heat up to 820°C for 5h, continue to heat up to 900°C, and heat for 15h. And receive the distilled lanthanum bromide to obtain high-purity anhydrous lanthanum bromide. After testing, the oxygen content in the high-purity anhydrous lanthanum bromide product of this example is 36 ppm, and the water content is 18 ppm.

[0034] The process flow diagram of this embodiment after obtaining thick anhydrous lanthanum bromide is shown in figure 1 .

Embodiment 2

[0036] Weigh 1 kg of cerium carbonate, add it gradually and completely dissolve it in a certain amount of commercially available concentrated hydrochloric acid (cerium carbonate and concentrated hydrochloric acid are added in a stoichiometric ratio), until the pH of the solution is 5-7, heat to 130°C to concentrate and crystallize Obtain cerium chloride hydrate crystals, transfer the obtained cerium chloride hydrate crystals to a vacuum device, and treat at 250°C for 10 hours to obtain crude anhydrous cerium chloride; transfer the crude anhydrous cerium chloride to a vacuum distillation device, and vacuumize Afterwards (vacuum pressure is 1100Pa at this moment) be warming up to 230 DEG C of insulation 5h, continue to heat up to 500 DEG C of insulation 4h, continue to heat up to 835 DEG C of insulation 5h, continue to heat up to 940 DEG C, insulation 15h, and receive distilled cerium chloride, Obtain high-purity anhydrous cerium chloride. After testing, the oxygen content in th...

Embodiment 3

[0038] Weigh 1.5kg of lanthanum oxide, add it gradually and completely dissolve it in a certain amount of commercially available concentrated hydrochloric acid (adding lanthanum oxide and concentrated hydrochloric acid according to the stoichiometric ratio), until the pH of the solution is 5-7, heat to 135°C Concentrate and crystallize to obtain hydrated lanthanum chloride crystals, transfer the obtained hydrated lanthanum chloride crystals to a vacuum device, protect the flow of Ar gas, and treat at 260 ° C for 10 hours to obtain crude anhydrous lanthanum chloride; transfer the crude anhydrous lanthanum chloride to In the vacuum distillation device, after vacuuming (at this time, the vacuum pressure is 12Pa), the temperature is raised to 300°C for 5 hours, and then the temperature is raised to 550°C for 3.5 hours, and then the temperature is raised to 865°C for 5 hours, and the temperature is continued to 1000°C for 18 hours. Receive the distilled lanthanum chloride to obtain ...

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Abstract

The invention provides a preparation method of high-quality anhydrous rare earth chloride and bromide. The preparation method comprises the following steps: (1) carrying out pre-dehydration on the rare earth halide REX<3>-xH<2>O to obtain crude anhydrous REX<3>, wherein X is elemental Br and/or Cl, RE is any one rare earth element or two or more rare earth elements consisting of Y, Sc, La, Ce, Pr,Nd, Sm, Pm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu, and x is no less than 0 and no more than 7; (2) vacuumizing the crude anhydrous REX<3> obtained in the step (1) under water-isolated and oxygen-isolated conditions; and (3) carrying out gradient heating on a system formed in the step (2) in a plurality of stages from 200-1500 DEG C, and carrying out distillation purification on the target objectREX<3> to obtain the high-purity anhydrous REX<3> with the absolute purity of more than or equal to 99.99%. According to the preparation method of the high-quality anhydrous rare earth chloride and bromide, different substances in a material are separated through process control, so the anhydrous rare earth halide with extremely high absolute purity is obtained; and the preparation method is relatively low in process cost, and easy for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic materials, in particular to a method for preparing high-quality anhydrous rare earth chlorides and bromides. Background technique [0002] Scintillation crystals are a type of crystals that emit visible light or ultraviolet light under the action of rays (X-rays, α-rays, β-rays) or high-energy particles (neutrons, etc.). It has a wide range of applications in exploration wells, non-destructive testing, safety inspections, etc. [0003] In the past 20 years, the research on halide scintillators has developed rapidly, and a large number of new scintillation crystals with high light output, good energy resolution or the ability to distinguish gamma and neutrons have emerged successively. Among them, LaBr 3 : Ce 3+ and LaCl 3 : Ce 3+ The representative rare earth halide scintillator materials have attracted widespread attention due to their high light efficiency, fast decay, high energy re...

Claims

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Application Information

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IPC IPC(8): C01F17/00
CPCC01P2006/80C01P2006/82
Inventor 段西健温永清张瑞森张志宏赵长玉张呈祥郝先库张瑞祥杨占峰
Owner TIANJIN BAOGANG RES INST OF RARE EARTHS
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